JP6120875B2 - 機械的表面活性化を使用してパラジウム−銀合金ガス分離膜を調製する方法 - Google Patents
機械的表面活性化を使用してパラジウム−銀合金ガス分離膜を調製する方法 Download PDFInfo
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- JP6120875B2 JP6120875B2 JP2014549170A JP2014549170A JP6120875B2 JP 6120875 B2 JP6120875 B2 JP 6120875B2 JP 2014549170 A JP2014549170 A JP 2014549170A JP 2014549170 A JP2014549170 A JP 2014549170A JP 6120875 B2 JP6120875 B2 JP 6120875B2
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- palladium
- silver
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Classifications
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- B01D67/0076—Pretreatment of inorganic membrane material prior to membrane formation, e.g. coating of metal powder
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
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- B01D67/0053—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/0055—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
- C01B3/503—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion characterised by the membrane
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1651—Two or more layers only obtained by electroless plating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble metals
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- C—CHEMISTRY; METALLURGY
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
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- C—CHEMISTRY; METALLURGY
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/48—Coating with alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/16—Hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/108—Hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
- B01D2323/081—Heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/04—Characteristic thickness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
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- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
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Description
本発明は、高価で時間がかかる化学的活性化を行わずに銀の上層および/またはパラジウムの追加層を施用しやすくするための、パラジウムの表面を活性化する安価で効率の高い方法を提供する。
本実施例は、金属間拡散バリアで被覆された多孔質基材の上に堆積された1層以上のパラジウム層の上に、1層以上の銀層を堆積させることを含む本発明の方法を利用する、パラジウムおよび銀を含有するガス分離膜システムの製造を例示する。
Mott corp.製の6インチのInconel 625多孔質支持体を、イットリア安定化ジルコニアの金属間拡散バリアで被覆し、50℃、5〜7インチのHgでパラジウムめっき液に支持体を通すことによって付着させた。金属間拡散バリアを含有するこの多孔質管を、洗浄し、乾燥し、その後、第1のめっきステップでめっきした。パラジウムおよび銀の膜を、7回のめっきステップで調製した。金属は次の順番でめっきされた:
1)パラジウム
2)銀
3)パラジウム
4)銀
5)パラジウム
6)パラジウム
7)パラジウム
Claims (14)
- パラジウム−銀合金ガス分離膜システムを調製する方法であって、
パラジウムを含む層を支持する多孔質支持体を用意するステップ;
前記パラジウム層を研磨媒体で研磨して、研磨模様および0.85ミクロンから2.5ミクロンまでの平均表面粗さ(Sa)を付すことによって、前記パラジウム層の表面を活性化するステップ;
前記活性化パラジウム層の表面上に、化学的活性化を行わずに、前記活性化パラジウム層の表面上にめっきされる銀を含む上層を堆積させるステップ;ならびに
400℃と800℃の間の温度で前記パラジウム層および銀の上層をアニールするステップ
を含む方法。 - 銀の上層を堆積させる前に、パラジウム層が0.85ミクロンから1.5ミクロンの範囲内の平均表面粗さ(Sa)に研磨される、請求項1に記載の方法。
- 銀の上層をめっきする前に、パラジウム層が、0.9ミクロンから1.2ミクロンの範囲内の平均表面粗さ(Sa)に研磨される、請求項1または2に記載の方法。
- 金属間拡散バリアが多孔質基材に施用され、前記多孔質基材とパラジウム層の間に配置される、請求項1から請求項3のいずれか一項に記載の方法。
- パラジウム層を堆積させる前に、銀の層が金属間拡散バリア上に堆積される、請求項4に記載の方法。
- 銀層上にパラジウム層を堆積させる前に、金属間拡散バリア上に堆積された前記銀層が0.85ミクロンと1.5ミクロンの間の平均表面粗さ(Sa)に研磨されることによって活性化される、請求項5に記載の方法。
- 堆積される銀の量が、全パラジウム層の1wt%から35wt%の間である、請求項1から請求項6のいずれか一項に記載の方法。
- パラジウム層が、1から10ミクロンの粒径を有する研磨媒体で研磨される、請求項1から請求項7のいずれか一項に記載の方法。
- 活性化パラジウム層上に堆積される銀の上層が、0.01ミクロンと10ミクロンの間の厚さを有する、請求項1から請求項8のいずれか一項に記載の方法。
- 0.8ミクロンより大きく2.5ミクロンまでの表面粗さ(Sa)に研磨することによって銀の上層を活性化した後、さらなるパラジウム層が前記銀の上層上に堆積される、請求項1から請求項9のいずれか一項に記載の方法。
- パラジウム−銀合金膜が0.001ミクロンから10ミクロンの厚さを有する、請求項1から請求項10のいずれか一項に記載の方法。
- 活性化パラジウム層上に堆積された銀の上層が、1ミクロンと2ミクロンの間の厚さを有する、請求項1から請求項11のいずれか一項に記載の方法。
- 銀の上層が、めっき液を循環させない無電解めっきによって堆積される、請求項1から請求項12のいずれか一項に記載の方法。
- 水素を水素含有ガス混合物から分離する方法であって、
パラジウム−銀合金ガス分離膜を、請求項1から13のいずれか一項に記載の方法により調製するステップ、および
前記ガス混合物を、前記パラジウム−銀合金ガス分離膜に通すステップ、
を含む方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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US201161577761P | 2011-12-20 | 2011-12-20 | |
US61/577,761 | 2011-12-20 | ||
PCT/US2012/070065 WO2013096184A1 (en) | 2011-12-20 | 2012-12-17 | A method of preparing a palladium- silver alloy gas separation membrane using mechanical surface activation |
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JP2015509040A JP2015509040A (ja) | 2015-03-26 |
JP6120875B2 true JP6120875B2 (ja) | 2017-04-26 |
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US (1) | US8876949B2 (ja) |
EP (1) | EP2794079A1 (ja) |
JP (1) | JP6120875B2 (ja) |
KR (1) | KR20140108644A (ja) |
CN (1) | CN104010719B (ja) |
CA (1) | CA2858597A1 (ja) |
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US20140251131A1 (en) * | 2013-03-07 | 2014-09-11 | James Douglas Way | Palladium-alloyed membranes and methods of making and using the same |
EP3129131B1 (en) * | 2014-04-10 | 2020-05-06 | Shell International Research Maatschappij B.V. | A method of making a supported gas separation membrane |
WO2015157414A1 (en) * | 2014-04-10 | 2015-10-15 | Shell Oil Company | A method of making a supported gas separation membrane |
US9987612B1 (en) | 2017-04-13 | 2018-06-05 | Caterpillar Inc. | Reactor assembly |
US11583810B2 (en) | 2020-12-14 | 2023-02-21 | Industrial Technology Research Institute | Porous substrate structure and manufacturing method thereof |
JP2024023015A (ja) * | 2022-08-08 | 2024-02-21 | トヨタ自動車株式会社 | 水素分離フィルター |
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US6152987A (en) * | 1997-12-15 | 2000-11-28 | Worcester Polytechnic Institute | Hydrogen gas-extraction module and method of fabrication |
AU2004224371B2 (en) | 2003-03-21 | 2008-07-31 | Worcester Polytechnic Institute | Method for fabricating composite gas separation modules |
JP2006520686A (ja) * | 2003-03-21 | 2006-09-14 | ウスター ポリテクニック インスティチュート | 中間金属層を有する複合ガス分離モジュール |
US7959711B2 (en) * | 2006-11-08 | 2011-06-14 | Shell Oil Company | Gas separation membrane system and method of making thereof using nanoscale metal material |
US7744675B2 (en) | 2006-11-08 | 2010-06-29 | Shell Oil Company | Gas separation membrane comprising a substrate with a layer of coated inorganic oxide particles and an overlayer of a gas-selective material, and its manufacture and use |
US8048199B2 (en) * | 2007-02-20 | 2011-11-01 | Shell Oil Company | Method of making a leak stable gas separation membrane system |
EP2125166B1 (en) | 2007-02-20 | 2014-06-25 | Shell Internationale Research Maatschappij B.V. | A method of reconditioning a gas separation membrane |
KR20130008033A (ko) * | 2010-03-26 | 2013-01-21 | 쉘 인터내셔날 리써취 마트샤피지 비.브이. | 지지된 가스 분리 멤브레인을 형성하는 방법 및 장치 |
US8721773B2 (en) * | 2011-10-26 | 2014-05-13 | Shell Oil Company | Method for preparing a palladium-gold alloy gas separation membrane system |
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- 2012-12-17 CA CA2858597A patent/CA2858597A1/en not_active Abandoned
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- 2012-12-17 JP JP2014549170A patent/JP6120875B2/ja not_active Expired - Fee Related
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- 2012-12-17 EP EP12809961.1A patent/EP2794079A1/en not_active Ceased
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CA2858597A1 (en) | 2013-06-27 |
TW201332631A (zh) | 2013-08-16 |
CN104010719B (zh) | 2016-06-01 |
JP2015509040A (ja) | 2015-03-26 |
KR20140108644A (ko) | 2014-09-12 |
US20130152785A1 (en) | 2013-06-20 |
WO2013096184A1 (en) | 2013-06-27 |
US8876949B2 (en) | 2014-11-04 |
CN104010719A (zh) | 2014-08-27 |
EP2794079A1 (en) | 2014-10-29 |
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